Process of cleaning wool.



No. 630,295.- Patented Aug. I, I899.

- E. MAERTENS.

PROCESS OF CLEANING WOOL.

(Application filed June 24, 1899.)

(No Model.)

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UNITED STATES PATENT GFFICE EMILE MAERTENS, OF PROVIDENCE, RHODE ISLAND.

PROCESS OF CLEANING WOOL.

SPECIFICATION forming part of Letters Patent No. 630,295, dated August 1, 1899;

Application filed June 24, 1899. Serial No. 721,732. (No specimens.)

To all whom it may concern:

Be it known that I, EMILE MAER'rEn's, a citizen of the United States, residing at Providence, in the county of Providence and State of Rhode Island, have invented certain new and useful improvements in the art of cleaning wool and other animal fibers with volatile solvents, the object being to obtain the wool or fiber in the best workable condition and to recover the by-products, such as Wool-fat and the potash, of which the following is a specification.

The invention relatesmore specifically to the process of removing the residual solvent which remains in the material under treatment after the fatty, oily, resinous, or other matters have been extracted therefrom and is designed for use in establishments where the output does not warrant the necessary expenditure for the more elaborate processes and apparatus described in my United States Patents Nos. 545,899, 545,900, and 615,030.

Referring to the accompanying drawings, Figure 1 isfa general elevation of the apparatus with the digester shown in section. Fig. 2 is a detail of thedigester-cover, and Fig. 3 is a detail of the hydraulic plunger with its perforated extension or platen.

A is the digester, wherein the material to be extracted is placed,eitherwhile contained in a cage or basket or loose, and is supposed to be provided with suitable doors or covers for loading and unloading the material and closing the apparatus. It can also be of the special construction shown herein, which consists of the straight cylindrical part a, carrying at its top an enlarged annular chamber a, adapted for the reception of a cover I) and of heating-coils c, and at its bottom a somewhat similar enlarged annular chamber d ada-ptedfor the reception of heating-coils c and of a hydraulic ram 01, having a watertight packing at e. The cover 17 consists of the solid cap part b and of the foraminous hollow extension b The ram (1, which is shown in detail in Fig. 3, consists of the plunger d (adapted to slide in the extension a of chamber a and of the foraminous' hollow extension or platen 61 which is fastened to it.

B is a reservoirprovided with suitable heating-coils for the solvent used in the process and when in use generally contains solvent having a certain amount of extracted matter in solution.

C isa condenser or cooler of any suitable construction for the cooling of liquids or the condensation of vapors.

D is a heater of any suitable construction for the heating or superheatiug of gases or vapors.

E is a vacuum-pump adapted for use also as an air or gas circulating pump, and it is connected by suitable valved piping with all the other elements of the apparatus.

F is an oil condenser or extractor used for the retention or condensation of the solvent vapors contained in the air which is allowed to escape into the atmosphere, and may be provided with heating means for the volatilization of the solvent retained by the oil in said condenser.

G and H are drums or reservoirs provided with heating-coils and are adapted for the reception of liquids for their separation, volatilization, or evaporation.

The various elements of the apparatus are provided wherever necessary with suitable valved inlet and outlet pipes, as well as with gages, drain -cocks, thermometers, sightglasses, &c.

The method for operating the apparatus is as follows, the material to be extracted or treated being supposedly raw wool: The dige'ster A having been charged with the wool to be extracted (in spaced) and hermetically sealed, by preference, and in order to insure a perfect penetration of the solvent to be used to all parts of the mass to be treated, a vacuum is created in the digester A by putting the latter in communication with the pump E through valve 1, pipes 100 and 101, and valve 2. The air exhausted is' discharged into the atmosphere through pipe 102 and valve 3. When a suitable vacuum has been obtained,the pump E is stopped and the valves previously opened are again closed. Steam having been turned onto the coils in' reservoir B by opening valve 4 on pipe 103, the pressure soon rises in this tank, through the tension of the vapors of the solvent volatilized by the heat of the coils, and when the internal pressure becomes'sufficient valve 6 on pipe 104,valves 7, 8, and 9 on pipe 105, and

valve'10 on pipe 106 are opened, or if the sola vent is judged to be too hot it is first put through the cooler or condenser via pipe 107, valve 11, pipe 108, and valve 12, and from the condenser enters pipe 105 by way of valve 13 on pipe 109 and valve 14 on pipe 110. When driving the solvent into pipe 105 by way of the condenser O, valve 7 on pipe 105 must of course be closed. The solvent containing extracted wool-fat in solution from preceding operations is now forced from the bottom of the tank B through the pipes and valves just mentioned into the top of the digester A, which is filled therewith. Should a vacuum not have been made in the digester prior to the admission of the solvent, the latter is preferably allowed to enterat the bottom of the digester by valve 38, the air displaced by the solvent being allowed to escape by opening valves 2 and 15 on pipe 101 and valve 16 on pipe 111 and enter the oil-condenser F through check valve 17, where in passing through the oil contained therein it is stripped of the solvent vapors with which it is charged before escaping intothe atmosphere through valve 18 on pipe 112, or it can first be-passed through the condenser O and from there to the condenser F by way of valves 19 and. 20 on pipe 113, valve 21 on pipe 114, pipe 115 and'valve 22 and check-valve 17 on pipe 111. The digester A being now full of solvent containing wool-fat in solution, valve 6 on pipe 104 is closed, valve 23 on pipe 116 is. opened, and valve 7 on pipe 105 is closed. The solvent vapors generated in reservoir B. now rise through pipes 116 104 107, valve 11, pipe 108, and valve 12 and enter the condenser through pipe'114, from which they emerge in liquid form through pipe 109, and from there the pure solvent enters the top of digester A throughvalve 13, pipe 110, valve 14, pipe 105, and valves 8, 9, and 10, valve 38 being closed. Valve 24 on pipe 117 and valve 25 on pipe 119 are now opened, and the charged solvent contained in digester A is allowed to return to tank B through pipes 117, 118, and 119, care being taken by throttling valves 24 or 25 not to let the charged solvent from the bottom of digester A into tank B-any faster than the pure solvent from condenser C enters digester A at its top, and thus acomplete continued immersion of the material being extracted is insured. If desired,,the solvent from the digester can be run into drums H orG by opening valves 28 or 40 before being returned to tank B. When the whole of the material contained in digester A has been sufficiently rinsed with the pure solvent coming from condenser G, valve 11 on pipe 107 is closed, as well as valves 12 and 13 on the inlet and the outlet to the condenser O, and valve 8 on pipe 105, whereas valve 7 on pipe 105, valve 26 on pipe109, valve 27 on pipe 120 are opened, valve 14 on pipe 110 not having been closed. Meanwhile all the liquid solvent contained in the digester A having been drained into tank B, valve 25 on pipe 119 is closed. The vapors generated in B now pass into the heater D,

where they are superheated, and from there through valve 10 into the top of the digester,

or they can be sent direct from pipe 104 into pipe 105 through valves 7, 8, 9, and 10 and be superheated in the chamber a by the coils 0. These superheated vapors which are under pressure somewhat compress the whole mass of wool and at the same time heat it up to the point of vaporization of the residual solvent which itcontains, and upon opening valve 28 on pipe 121, leading into drum G, a quantity of liquid solvent is discharged into said drum, whereas vaporized solvent ascends pipe 122 into pipe 101, and from'there enters the condenser by way of valve 15, pipe 113, valve 19, pipe 108, valve 12, and pipe 114, and when condensed is delivered into drum H or G via valve 29 on'pipe- 123 andvalves 30 and 31. Thisoperation is continued until substantially all the residual solventhasbeen removed from the-material. I have found'by experience that the wool is liable to be injured it in the treatment thereof the temperature is allowed to go above centj grade. The exact temperature will vary with different wools, as well as with the nature of the solvent employed. The temperature which I prefer to employ in driving off the residual-solvent from the wool is from 50 to 55 centigrade. Valves 4, 23, 9, and 28 are now closed, steam is turned on at valve 32 on pipe 106 for a few seconds, and this completely removes the last traces of solvent. and deodorizes the material, which is now dry and degreased and in condition for removal from the digester in any suitable manner after atmospheric air has been circulated through the material in order tocool it off. This is done by closing all valves pump, and openingvalve 3 on pipe 102, valve 1 on pipe 100, valve 2 on pipe 101, and valve 33 on pipe 124. This latter valve 33 admits atmospheric air, which is drawn through'the mass and discharged into the atmosphere either through valve 3 or by way of the oilcondenser F via valves 34 and 22 on pipe 115 and valve 18 on pipe 112 or by way of condenser C and the oil-condenser F, as previously described.

The removal of residual solvent by the aid of superheated solvent vapors alone is a tedious and dangerous operation, which unless carried on with great care and judgment is very liable to injure the material being treated when this is wool and is not to be recommended even if carried on by very experienced and careful operators.

Theremoval of the residual solvent'is much accelerated, the quality of the work is much improved, and the danger of injury to the material very materially removed by the use of a vacuum-pump or of steam in conjunction with solvent vapors or by a combination of two or of all three of the elements mentioned.

previously opened, starting up the vacuum- IIO When steam is used with or without the vacuum-pump, a small jet of it is admitted to pipe 106 by valve 32, where it mixes with the solvent vapors before they enter the digester, the water resulting from the condensation of the steam being separated from the solvent in drums H or G.

When the vacuum-pump is used with solvent vapors or with steam, or with both solvent vapors and steam, for the removal of the residual solvent, valve 28 on pipe 121 is closed, and all other valves being open or shut as required the vapors are circulated from the bottom of the digester through valve 24. on pipe 117, through pipes 122, 101, 100, and through valve 1, and are discharged by the pump E into condenser 0 via pipe 102, valve 34, pipe 115, and valve 21 on pipe 114, the liquefied vapors finding their way into drums II or G via pipe 109, valve 29, pipe 120, and valves 30 or 31.

In lieu of solvent vapors water-vapors are sometimes used for the removal of the residual solvent, and when this is the case valve 24 on pipe 117 is closed, and the bottom chamber a of the digester is filled or partially filled with water by opening valves 35 and 36 on pipe 125. Steam is turned on to coils c of chamber a by opening valve 37, valve 2 on pipe 101 and valve 1 on pipe being opened and the vacuum-pump started. Under the influence of the vacuum produced and the heat transmitted by coils c the waterin chamber a is vaporized and drawn through the contents of the digester,heating it up and vaporizin g the residual solvent, which along with the water-vapors is delivered by the pump E into condenser Cand from there into drums II or G, as previously described.

In lieu of water-vapors, of steam, of solvent vapors, or a combination of two or three of the above, with or without a vacuum, the residual solvent is sometimes removed by air, which is circulated over and over again through the material, preferably in conjunction with steam. When this is practiced, air is allowed to enter the system by valve 33 on pipe 124 or by any other inlet or inlets suitably situated for the purpose, and the pump E is started. If desired, the air may be indirectly heated prior to its introduction into the digester or may be directly heated by mixin g steam therewith. The air is drawn through the material and emerges from the digester through valve 2 on pipe 101, enters the pump through Valve 1 on pipe 100, leaves the pump through pipe 102, enters the condenser through valve 34 on pipe and valve 21 on pipe 114, passes through the condenser, (leaving behind solvent and water vapors, which are condensed and run to tanks H or G via valve 29 on pipe 123 and valves 30 or 31,) and through pipe 109 and valves 13 and 26 enters the heater D, where it absorbs heat, emerges from the latter through pipe 120, and enters pipe 105 through valve 27and pipe 106 through valve 9. In pipe 106 it is preferably mixed 'with steam injected through valve 32 and reenters the bottom chamber a of digester A through valve 38. This air is thus circulated in a cycle, recooled, reheated, and remixed with steam.until all of the residual solvent contained in the material held by the digester has been removed, and it is then discharged into the atmosphere by way of the oil-condenser, as previously described.

In order to accelerate the removal of the residual solvent and before the circulation of steam, air, or vapors through the material, the latter can be squeezed for the expression of the bulk of the residual solvent. This is accomplished by making use of the ram (1, (orof any equivalent deviceIormeansQ which on being raised by the medium actuating it compresses the material between the hollow foraminous platen d and the hollow foraminous extension 12 of the coverb, the liquid expressed escaping through the perforations of said platen and cover into chambers a? and a and emerging from there through valves 10 and 38 on pipe 106 and valves 24 and 28 on pipe 117 and. 121 into drum G. When the liquid has been expressed, as described, the ram is again allowed to drop and the removal of the still adhering solvent is carried on as previously described.

'It is obvious that after treating the material and removing the cover I) the digester can be emptied by the action of the plunger (1', which when raised carries with it the hollow foraminous platen d and all that is supported by the latter to the top of the digester A, where it is cared for in any suitable manner.

When the material being extracted is going to be subjected to a subsequent wet treatment in the digester itself, it is convenient to remove the residual solvent by means of the liquid or solution with which the material is to be treated or with water, provided these are immiscible with the solvent used in the extraction, and the operation is then as follows: Assuming that the liquid to be used is water and that the material is to be partially prepared for carbonizing or entirely carbonized in the digester A and that the bulk of the residual solvent has or has not been removed by compression, as described above, Water of a suitable temperature is allowed to enter digester A via valve 36, pipe 125,valve 35, and chamber a, (it can, if need be, be heated by coils c' in said chamber) and to rise slowly in the part a, containing the extracted material. The adhering solvent is thereby nearly all removed and floated on top of the Water or solution used. When the floating solvent reaches chamber b the inlet flow of water is reduced or stopped, steam is turned on the coil 0 by opening valve 39, and the floating solvent distilled off either in vacuo, the vapors going through valves 2 and 1 and the pump on their way to the condenser or direct to the condenser via valve 2, pipe 101, valve 15,'pipes 104 and 113, valve 19, pipe 108,, and valve 12, or the solvent canbe floated om slowly into-drumsI-l or Gvia valve been removed,.valve 2-isiclosed and the materiali's'compressed by moving-plunger dv upward,aspreviously'described: This liberates:

furthertracesof' solvent and also-the natural soaps or potash salts: contained inthe'wool and whichhad dissolved in the surrounding liquid. The floating solvent is floated ofi or distilled 0%, as previously described,.and the liquid containing. the potash salts insolntion.

is run into drums H or G by Way of. valves 10 andr38 on pipe 106 andvalve 24, pipe-117,, and valves28: or40forthe removal of traces of solvent, oritisrun direct to a storage-tank .5

byway of Valve 33Jon. pipe 124 for reuseor until its concentration: warrants: its vaporization for the recovery of the potash salts or other extracted material held in solution. Thematerialfcanmow after a slight steaming be removed from the digester and carriedto the'washers' to be rinsed for the removalofextraneousdmpurities, or it can be further rinsed in the digester itself by repeated; immersions, compressions, and'changes. of water, andthis is the case when it-issdesiredto prepare the material for carbonizing'or when it is desired to carbonize the material in the digesteritselfor'to remove-it from the digester' cleansed or cleansed and dried.

In order to prepare the material for'carrbone' izing, after it has been sufiiciently rinsed it is finally compressed and the water allowed: to drain. out. of the digester through valve 33 on pipe 124:. The plunger d is then allowed'to drop, and after closing'valve 33 the carbonizingisolution is introduced through valve i l and 35 on pipe 125 and chamber a intothe port-a of digester A. When the material-contained therein is completely immersed by the solution, the flow is-stopped, and the mate rial issallowed to steep for alsuitableperiod'. Thesolution-is then. allowed toretnrnto its storage-tank through valve 33 onpipe'124, and the plunger (1 is made to compress the material for the removal of the bulk of the adheringcarbonizingsolution. Themater-ial can-now be removedto be dried, carbonized; neutralized, and 'redried, or it can be driedby passing steam and hot air. through it' in the 9 manner previously described and when dry carbonizedby eliminating the steam from the circulation.and-increasing the temperature of the circulating airin-the heaterD and in coils c i and-c.

When the carbonization is complete, the material can be neutralized in the same inanner that it was prepared for the carbonization by merely changing the solution used.

plunger 01.

idrums H and Gare separated by-decantation tor evaporation,,or by both, the drums being isuitably connected with the condenser G. and tank B, as well as with the drain andwith-ston Eage-tanks,-. for this purpose. 7

If desired,- the material can be treatedwith water in the digester aft-er the residual sol- ;}vent has been removed by superheated sol-' {event vapors,-w-ater-vapors, air or steam; or fbOtll, or a combination of any of the means i; mentioned. If this water treatment is' done f thoroughly in the case of some wools, so asto removezall potas-h soaps present, andzthe wool zzisthen' partially dried, it canthen in many Kcasesbe freely carded, and an expensive proc= less can thus be saved.

much-saturated withextracted fat, a part of it T; istrun to a still; where the fatisrseparated from @the-sollvent. The solvent istlien returned to gtank B by way of the-condenser 0 direct, or by way of. condenser O and drums and G "in case the solvent is mixed with water and .needs separating in's'aid: drums.

It is evident from the description and'drawii'ngsthanif desired,.the liquids, gases,.or vaipors used in the'process can beipassed through Ethe digester in either direction when itis lideemed advisable'or necessary to so-do. It is evident. that the vacuum-pump can be distdensed with,.if necessary, in some-0t the opierationsdescribed and that the suction or vacuum created by the condensation of the vapors in the condenser will to a great extent ia-ecomplishthesameobject. Itisafurtherevident that when'thesolvent used in the process is heavier than/ the extracted matter its fflow through the digestershould beupward, whereas when the solvent islighter than the giextracted matter-itsflow should be downward, fiand'that in case ofsthe removal of the residual isolvent with a liquid the flow of the liquid gshould bedownward if the solvent is heavier ;than theliquid used for its removal and that i the flow of said liquid should beupward through the digesterwhen. the solvent is ilighter than the liquid usedfor itsv removal. The method hereinbeforedescribed of relmoving residual solvent: by superheated sol- -vent vaporsis claimed in my application SerialNo. 721,730.

The described method of removing residual solvent by the circulation of air in a closed circuit is claimedin my application Serial No. 721,731.

The'described method of removing residual solvent: by the inflow of water is-claimed in my application Serial'No. 721,733.

Having described my invention, what I claim is 1. The improved method of removing residualsolvent from wool (and other material) in gaseous or vapor form which consists in subjecting it to the action of steam or aqueous vapor in conjunction with a vacuum at -.a temperature not-exceeding 100 centigrade, isubstantially as described.

2. The improved method of removing residual solvent from wool (and other material) in gaseous or vapor form which consists in subjecting it to the action of steam in conjunction with a vacuum at a temperature below the point at which the material would be injured by heat, substantially as described.

3. The improved method of removing residual solvent from wool (and other material) in gaseous or vapor form which consists in passing steam or aqueous vapor through it at a temperature below the point at which the material would be injured by the heat.

4. The improved method of removing residual solvent from wool (and other material) in gaseous or vapor form which consists in subjecting it to the action of aqueous vapor in conjunction with a vacuum, substantially as described.

5. The improved method of removing residual solvent from wool (and other material) in gaseous or vapor form which consists in passing aqueous vapor through it at a temperature below the point at which the material would be injured by the heat, substantially as described.

6. The improved method of treating wool which consists in subjecting it to the action of steam or aqueous vapor in conjunction with a vacuum at a temperature not exceeding 100 centigrade to volatilize the residual solvent therefrom and then removing the potash or potash salts, therefrom, substantially as described.

7. The improved method of treating wool which consists in subjecting it to the action of aqueous vapor in conjunction with a vacuum at a temperature not exceeding 100 centi grade to volatilize the residual solvent therefrom and then removing the potash or potash salts therefrom, substantially as described.

8. The improved method of treating wool which consists in passing steam through it at a temperature below the point at which the material would be injured by the heat, to volatilize the resid ual solvent therefrom then Washing it, and finally drying it, substantially as described.

9. The improved method of treating wool which consists in passing aqueous vapor through it at a temperature below the point at which the material would be injured by the heat, to volatilize the residual solvent therefrom then washing it, and finallydryi ng it, substantially as described.

10. The method of removing residual solvent from wool which consists in subjecting it to the action of aqueous vapor at'a tem p erature not exceeding 60 centigrade.

EMILE MAERTENS.

Witnesses:

MABEL I. FAY, RUFUS S. MATTEsoN. 

